It is known in the art of high pressure fluid or supercritical fluid restrictors to restrict the flow of fluid with fluid restrictors instead of valves because the fluid flow rates, which can be in the range of 10 microliters/min. to 10 ml/min., are too low for accurate and reproducible flow control by conventional valves.
In one type of fluid restrictor, holes are formed in a circular disc that are supported in the path of the flowing fluid by the necessary hardware, seals and fittings.
A problem exists with such fluid restrictors in that the small size of the hole and its abrupt change in cross sectional area allow it to become clogged easily. This is an undesirable event in that it typically entails dismounting the fluid restrictor so that it can be cleaned or replacing it altogether.
It is also known to use linear fused silica tubing having a small internal channel as a fluid restrictor. Tapered fused silica restrictors are also formed by heating and drawing out the fused silica tubing until the internal channel is the appropriate dimension. (T. L. Chester, D. P. Innis, G. D. Owens, Analytical Chemistry, 57 (1985) 2243-2247).
"Integral" fused silica restrictors (E. J. Guthrie, H. E. Schwartz, J. Chromatographic Science, 24 (1986) 236-241) are formed by heating the end of the fused silica tubing until it melts shut. Then, sending away the end until a small hole is formed Ceramic frits have also been formed at the ends of the fused silica restrictor (K. E. Morkides, S. M. Fields, M. L. Lee, J. Chromatographic Science, 24 (1986) 254-257). A review of restrictors is given by B. W. Wright, R. D. Smith, "Restrictor Performance Characteristics for SFC", Chapter 10 of Book Modern Supercritical Fluid Chromatography, Ed C. M. White, Dr. Alfred Huthig Verlag, ISBN 3-7785-1569-1, 1988.
A length of fused silica tubing does better as a restrictor than a hole in a disc as it plugs less often, but it is limited by other deficiencies including 1) it is brittle and can break easily, 2) one must use a long length, typically 10 to 100 centimeters which makes its use inconvenient to the user, and 3) since the tube is glass, it is a poor thermal insulator and thus it is difficult to heat. Heat has been shown to reduce clogging in fluid restrictors.
Fluid restrictors have also been constructed by crimping a stainless steel or platinum tube with pliers to deform the wall thereby decreasing the cross sectional area of the channel within. Though such restrictors are less prone to clogging, the pliers cause the outer diameter of the wall to become greater than its original value in places. This flaring of the tube prevents a snug fit in the appropriate fittings. Thus, efficient heat transfer is limited. A further problem exists in that it is difficult if not impossible to reproduce the shape or profile of the deformity. This limits the accuracy in predicting the magnitude of fluid restriction and the aversion to clogging.
The present invention provides a fluid restrictor wherein the wall is deformed such that the channel within is restricted without flaring of the walls and the deformity is reproducible. The operation of these restrictors occurs at temperatures of 50.degree. C. to 250.degree. C. to further reduce clogging.